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Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2017-03-13 to 2017-05-12
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2017
Report date:
2017

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry

Test material

Constituent 1
Chemical structure
Reference substance name:
1'-(phenylmethyl)-[1,4'-bipiperidine]-4'-carbonitrile
EC Number:
282-544-0
EC Name:
1'-(phenylmethyl)-[1,4'-bipiperidine]-4'-carbonitrile
Cas Number:
84254-97-7
Molecular formula:
C18H25N3
IUPAC Name:
1'-benzyl-[1,4'-bipiperidine]-4'-carbonitrile
Test material form:
solid: particulate/powder
Specific details on test material used for the study:
- Batch n°: I15IB3393
- Analytical purity: 99.93%
- Expiration date: 2017-10-25
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
106.1 °C
Atm. press.:
1 013.25 hPa
Decomposition:
yes
Remarks:
A dark yellow to orange/brown molten residue remained after the preliminary and main test, indicating reaction and/or decomposition.
Decomp. temp.:
> 150 °C

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 225°C. At 320°C the sample weight has decreased by 25%. After the experiment, an orange/brown molten residue remained in the sample container (original colour: beige). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

In order to determine the melting more precisely, the DSC curve with a heating rate of 20°C/min was obtained and showed an endothermic peak between 75°C and 125°C. The extrapolated onset temperature of the peak was 105.956°C. The effect was most likely obtained due to melting. A second endothermic peak was observed between 150°C and 320°C due to reaction and/or decomposition of the test item. After the experiment, a dark yellow molten residue remained. To investigate the melting peak between 75°C and 125°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 106.149°C. The melting temperature of T000745 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 106.1°C (379.2K).

Applicant's summary and conclusion

Conclusions:
The melting temperature of JNJ-1594983-AAA (T000745) was determined at 106.1°C (379.2K) by using DSC.